CN106033040A - Metal-based composite material shearing strength testing method and sample preparation method - Google Patents
Metal-based composite material shearing strength testing method and sample preparation method Download PDFInfo
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- CN106033040A CN106033040A CN201610051817.0A CN201610051817A CN106033040A CN 106033040 A CN106033040 A CN 106033040A CN 201610051817 A CN201610051817 A CN 201610051817A CN 106033040 A CN106033040 A CN 106033040A
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- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/24—Investigating strength properties of solid materials by application of mechanical stress by applying steady shearing forces
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Abstract
The invention relates to a metal-based composite material shearing strength testing method and a preparation method of a sample applied in the testing method. According to the principle, a micro-nano size cylinder containing a separate reinforcement-substrate interface is etched by means of focused ion beams, the reinforcement-substrate interface of the micro-nano size cylinder and the axial direction of the cylinder form a 45-degree angle, pressure is exerted on the top surface of the micro-nano size cylinder in the axial direction by using a nanoindentor, and the micro-nano size cylinder is compacted and deformed; in the process, the direction, forming 45 degrees with the compaction direction, of the reinforcement-substrate interface will bear the maximum shearing strength till the shear behavior occurs on the reinforcement-substrate interface, and the shearing strength of the reinforcement-substrate interface is calculated according to a stress-strain curve, recorded through the nanoindentor, of the micro-nano size cylinder.
Description
Technical field
The present invention relates to reinforcement and the method for matrix interface shear strength in a kind of Validity Test metal-base composites, and the preparation method of sample applied in this method of testing, belong to field of metal matrix composite.
Background technology
In metal-base composites interface between reinforcement and matrix be connect both " tie ", be mechanics and other function between the two, as heat conduction, conduct electricity, " bridge " of the characteristic transmission such as damping.Therefore, the character of interfacial structure, interface bond strength and interface microcell is the key affecting metal-base composites performance.But, structure and the combination of reinforcement-basal body interface are considerably complicated, and are highly dependent on the enhancing kind of phase, initial condition and preparation technology；On the other hand, scrambling due to reinforcement (the particularly discontinuous reinforcement such as granule, whisker body) shape, it is difficult to directly measure the bond strength of reinforcement-basal body interface by traditional experimental technique, thus greatly hinder the research to its compound interface response mechanism and explaination, and accurately intending real and calculating its performance.In order to solve this difficult problem, researcher typically requires sets up certain theoretical model, and carries out compareing and matching with model by the experimental result of macroscopic material, and then obtains interface bond strength.But, this kind of modeling and the often deformation mode to shape, distribution and the interface of reinforcement that calculates have carried out considerable degree of simplification and have processed.Such as, in conventional " adhesion zone model ", researcher generally assumes that reinforcement is spherical and arranges in periodic regular in matrix, by having identical reinforcement volume fraction but the matching of macroscopical sample stress strain curve of different reinforcement size, obtaining interface bond strength and Work of Adhesion；And in the simulation to fracture of composite materials behavior, reinforcement granule is approximately embedded to body two-dimensional disc by researcher, by the situation of disk upper stress distribution under the conditions of calculating uniaxial tensile stress, ask for the bond strength at interface.
nullAlthough people have carried out much work to study metal-base composites、The particularly structure of discontinuous phase reinforced metal based composites compound interface and bond strength，But main research work is only limitted to from the displaing microstructure observing at interface to speculate the situation of interface cohesion，And rely on specific hypothesis or simplified model，The interface bond strength with particular experiment data match is obtained by data matching with numerical computations under the conditions of certain model hypothesis，And still it is formed without effective ways and the technology of an energy Accurate Determining Metal Matrix Composite Interface bond strength，And wherein the preparation of test sample is the key of restriction test metal-base composites shear strength，How to prepare suitable test model、Set up quantitative test and the evaluation methodology of an effective interface bond strength，There is provided accurately with calculating for theoretical modeling、Directly quantitative data support the most just becomes those skilled in the art's technical issues that need to address with the coupled relation of explaination " interface-performance ".
Summary of the invention
The technical problem to be solved is to provide a kind of method of test metal-base composites shear strength directly, being easily achieved, and the preparation method of sample applied in this method of testing.
In order to solve the problems referred to above, the invention provides the method for testing of a kind of metal-base composites shear strength, its principle is, utilize focused ion bundle (Focus Ion Beam, FIB) the micro-or nano size cylinder containing single reinforcement-basal body interface is etched, and the reinforcement-basal body interface of this micro-or nano size cylinder axially has certain angle with this cylinder, then nano-hardness tester is used axially to apply pressure along it at the end face of micro-or nano size cylinder, so that micro-or nano size cylinder generation compressive deformation, shearing force will be born in reinforcement-basal body interface direction in the process, until shearing behavior will occur at reinforcement-basal body interface, the shear strength of reinforcement-basal body interface is calculated by the load-deformation curve of the micro-or nano size cylinder of nano-hardness tester record.This test, owing to sample bench taking in FIB cutting specimen artificial inclination, final obtains " little to not losing the performance of macrocomposite, big to testing and can process ", micro-or nano size cylinder sample containing independent reinforcement-basal body interface.
Further, described reinforcement-basal body interface angle axial with this micro-or nano size cylinder sample is 45 °, described micro-or nano size column diameter be 200nm to 10 μm, draw ratio be 2:1～6:1, the tapering of micro-or nano size cylinder end face is not more than 3 °, nano-hardness tester is during compression micro-or nano size cylinder sample so that during compression experiment, reinforcement-basal body interface is loaded by maximum shear component；After cylinder sample failure mode is carried out Reasonable Regulation And Control, reinforcement-basal body interface generation shearing slip when making compression verification, to record the bond strength at interface intuitively, easily；In test process, can take to increase stressed method step by step, and use scanning electron microscope (SEM), transmission electron microscope (TEM) to observe under the conditions of different compression stress before and after compression experiment reinforcement-basal body interface and the Characteristics of Microstructure of microcell thereof in micro-or nano size cylinder sample, thus judge whether reinforcement-basal body interface lost efficacy.
The preparation method of above-mentioned micro-or nano size cylinder, the metal-base composites of selection is aluminum-base silicon carbide, comprises the steps, with wire cutting machine, 4H-SiC single-chip cuts into 10*10 mm square pieces；According to ethanol, acetone, the sequencing of isopropanol, SiC single crystal small pieces are carried out each 10min ultrasonic cleaning, remove wafer surface impurity；SiC single crystal small pieces are immersed 700 DEG C of melted Al(purity 99.99%) in liquid, hand operated mixing 4S proposes, repeat above action until the thickness of Al layer is more than 1mm, prepare Al-SiC-Al sandwich structure composite；The one side selecting Al-SiC-Al sandwich structure composite sample is polished so that this face is smooth and Al aspect is parallel to SiC wafer；Composite sample after polishing is fixed on the wedge shape platform at 45 ° of inclination angles, and the one side of polishing is close to wedge shape microscope carrier；Sample parallel one side bottom wedge shape microscope carrier is polished, it is thus achieved that a plane being parallel to bottom；At sample parallel in the plane of foot wedges, utilize FIB to etch diameter 200nm to 10 μm, draw ratio is 2:1～6:1, the micro-or nano size cylinder of SiC-Al aspect ratio about 1:1, and the top tapering of micro-or nano size cylinder is less than 3 °, obtain " little to not losing the performance of macrocomposite, big to testing and can process ", micro-or nano size cylinder sample containing independent reinforcement-basal body interface.
The method of testing manufacture method of a kind of metal-base composites shear strength, comprises the following specific steps that:
A, select the metal-base composites of suitable dimension so that the size of the two phase material that reinforcement-basal body interface of being studied is corresponding can be used to prepare micro-or nano size cylinder, described reinforcement and matrix size and is in micron dimension.
B, use FIB etch there is independent reinforcement-basal body interface, this interface and cylinder axially have the micro-or nano size cylinder of certain angle.
C, according to the compression parameters preset, use the tack pressure head of nano-hardness tester axially to apply certain pressure at the end face of micro-or nano size cylinder along it, carry out stress-strain test, use the reinforcement after tem observation deformation-
Basal body interface, it is judged that whether reinforcement-basal body interface lost efficacy.
D, it is stepped up compression parameters, by the experimental result comparison under the conditions of different compression parameters, the shear strength between reinforcement and basal body interface can be recorded more accurately, draw the shear strength of reinforcement and basal body interface according to the significantly stress-strain sudden change occurred on load-deformation curve.
Further, in step B, described micro-or nano size column diameter be 200nm to 10 μm, draw ratio be 2:1～6:1, the tapering of micro-or nano size cylinder end face is not more than 3 °, so that test is easy to observe, it is to avoid the hardening of load-deformation curve, causes data distortion.
Further, described reinforcement and the biphase aspect ratio of matrix are about 1:1, so that test is easy to observe.
Further, in described step B, described reinforcement-basal body interface and this cylinder axially between angle be 45 °, the shear strength of described reinforcement-basal body interface is equal to a half value of the stress occurring catastrophe point on a large scale on load-deformation curve.
The technique effect of invention: test metal-base composites reinforcement and the method for matrix interface shear strength of (1) present invention, utilizes micro-nano mechanics method can directly record interface shear strength, overcomes the difficult problem that traditional method cannot directly record；(2) micro-or nano size cylinder design become the tilted interface the most at 45 ° with reinforcement-basal body interface shearing behavior can be made to be more prone to occur；(3) the end face tapering of micro-or nano size cylinder is not more than 3 °, it is to avoid the hardening of load-deformation curve, causes data distortion；(4) use step by step and be gradually increased the compress mode of decrement, the shear strength between reinforcement and basal body interface can be recorded more accurately；(5) use scanning electron microscope (SEM), transmission electron microscope (TEM) to characterize under the conditions of different compression stress before and after compression experiment reinforcement-basal body interface and the Characteristics of Microstructure of microcell thereof in micro-or nano size cylinder sample, can effectively result be verified.
Accompanying drawing explanation
Below in conjunction with Figure of description, the present invention is described in further detail:
Fig. 1 is the compression force analysis schematic diagram of SiC/Al micro-or nano size cylinder in the embodiment of the present invention；
Fig. 2 is the SEM shape appearance figure that the SiC/Al that in the embodiment of the present invention, FIB etches is combined microtrabeculae 1# sample；
Fig. 3 is the TEM shape appearance figure of the front reinforcement-basal body interface of SiC/Al micro-or nano size cylinder 1# sample contracting in the embodiment of the present invention；
Fig. 4 is that in the embodiment of the present invention, SiC/Al micro-or nano size cylinder 1# sample decrement is stress-strain curve when 7%；
Fig. 5 is the SEM shape appearance figure after SiC/Al micro-or nano size cylinder 1# sample decrement is 7% in the embodiment of the present invention；
In Fig. 6 embodiment of the present invention, SiC/Al micro-or nano size cylinder 1# sample decrement is stress-strain curve when 9%；
Fig. 7 is the SEM shape appearance figure after SiC/Al micro-or nano size cylinder 1# sample decrement is 9% in the embodiment of the present invention；
In Fig. 8 embodiment of the present invention, SiC/Al micro-or nano size cylinder 1# sample decrement is stress-strain curve when 11%；
Fig. 9 is the SEM shape appearance figure after SiC/Al micro-or nano size cylinder 1# sample decrement is 11% in the embodiment of the present invention；
The TEM pattern of reinforcement-basal body interface after SiC/Al micro-or nano size cylinder 1# sample lost efficacy in Figure 10 embodiment of the present invention；
Figure 11 is that in the embodiment of the present invention, SiC/Al micro-or nano size cylinder 2# sample decrement is stress-strain curve when 11%；
Figure 12 is that in the embodiment of the present invention, SiC/Al micro-or nano size cylinder 3# sample decrement is stress-strain curve when 11%；
Figure 13 is that in the embodiment of the present invention, SiC/Al micro-or nano size cylinder 4# sample decrement is stress-strain curve when 11%；
Figure 14 is that in the embodiment of the present invention, SiC/Al micro-or nano size cylinder 5# sample decrement is stress-strain curve when 11%.
Detailed description of the invention
Embodiment 1
Aluminum-base silicon carbide particulate reinforced composite fully combines the different advantages of silicon carbide ceramics and metallic aluminium, there is thermal coefficient of expansion, density that high-termal conductivity matches with chip little, lightweight, and high rigidity and high-flexural strength, it is the outstanding person in a new generation's electronic package material, meet the requirements such as the lighting of encapsulation, densification, be suitable to apply the fields such as Aeronautics and Astronautics, high ferro and microwave.The present embodiment is specifically described with aluminum-base silicon carbide (SiC/Al).
As shown in Figure 1, FIB is used to etch the micro-or nano size cylinder 1 containing single reinforcement-basal body interface 2, the sectional area of the end face 3 of this cylinder is A, reinforcement-basal body interface 2 angle axial with cylinder is θ, it is P at the end face 3 of cylinder along the pressure that cylinder axially applies, this cylinder is P/A along its axial pressure, reinforcement-
The sectional area of basal body interface 2 is A/ cos θ, this pressure makes micro-or nano size cylinder 1 axially be deformed along it, owing to being two combined structures at reinforcement-basal body interface, the stress of this junction will be little compared to the stress of independent Metal Substrate or independent reinforcement, therefore first produce strain at reinforcement-basal body interface to lose efficacy when pressure is sufficiently large, micro-or nano size cylinder 1 produces fracture along reinforcement-basal body interface 2 direction, and load-deformation curve produces and significantly suddenlys change；It is P*sin θ that this pressure edge at reinforcement-basal body interface 2 is parallel to the component in direction, interface, what this component acted on reinforcement-basal body interface 2 is P*sin θ/(A/ cos θ) along being parallel to the pressure (i.e. the shear strength of reinforcement-basal body interface) in direction, interface, i.e. P*sin θ * cos θ/A, when prepared by sample, guarantee that the axial angle theta of reinforcement-basal body interface 2 and cylinder is 45 °, therefore shear strength is this micro-or nano size cylinder axial compression strength 1/2 at this reinforcement-basal body interface 2.
The preparation of above-mentioned micro-or nano size cylinder 1: 4H-SiC single-chip cut into 10*10 mm square pieces with wire cutting machine；According to ethanol, acetone, the sequencing of isopropanol, SiC single crystal small pieces are carried out each 10min ultrasonic cleaning, remove wafer surface impurity；SiC single crystal small pieces are immersed 700 DEG C of melted Al(purity 99.99%) in liquid, hand operated mixing 4S proposes, repeat above action until the thickness of Al layer is more than 1mm, prepare Al-SiC-Al sandwich structure composite.The one side selecting Al-SiC-Al sandwich structure composite sample is polished so that this face is smooth and Al aspect is parallel to SiC wafer；Composite sample after polishing is fixed on the wedge shape platform at 45 ° of inclination angles, and the one side of polishing is close to wedge shape microscope carrier；Sample parallel one side bottom wedge shape microscope carrier is polished, it is thus achieved that a plane being parallel to bottom；At sample parallel in the plane of foot wedges, FIB is utilized to etch diameter about 1 μm, draw ratio 4:1, the micro-or nano size cylinder 1# sample of SiC-Al aspect ratio about 1:1, and the top tapering of micro-or nano size cylinder is less than 3 °, SEM is used to observe this micro-or nano size cylinder 1# sample, the SEM shape appearance figure such as Fig. 2 obtained, using the reinforcement-basal body interface 2 of this micro-or nano size cylinder 1# sample of tem observation, the TEM shape appearance figure obtained is as shown in Figure 3.
Utilize nano-hardness tester that micro-or nano size cylinder 1# sample is compressed experiment, deformation rate axial for cylinder is set as 7%, obtain load-deformation curve, as shown in Figure 4, can determine whether according to load-deformation curve now, reinforcement-basal body interface does not produce fracture, use SEM to observe micro-or nano size cylinder now, obtain SEM shape appearance figure, as shown in Figure 5, thus can confirm that, reinforcement-basal body interface does not produces fracture；Adjust nano-hardness tester, deformation rate axial for cylinder is set as 9%, again obtain load-deformation curve, as shown in Figure 6, can determine whether according to load-deformation curve now, reinforcement-basal body interface does not produces fracture yet, use SEM to observe micro-or nano size cylinder now, again obtain SEM shape appearance figure, as shown in Figure 7, thus can confirm that, reinforcement-basal body interface does not produces fracture yet；Again adjust nano-hardness tester, deformation rate axial for cylinder is set as 11%, again obtain load-deformation curve, as shown in Figure 8, load-deformation curve now produces sudden change, thus judge that reinforcement-basal body interface does not produces fracture, SEM is used to observe micro-or nano size cylinder now, obtain SEM shape appearance figure, as shown in Figure 9, reinforcement-basal body interface produces fracture, re-use and be amplified observing at the TEM strong body-basal body interface to the micro-or nano size cylinder after compression, the TEM shape appearance figure obtained is as shown in Figure 10, thus can confirm that reinforcement-basal body interface ruptures really, lost efficacy.
The size micro-or nano size cylinder 2# sample essentially identical with micro-or nano size cylinder 1# specimen size, micro-or nano size cylinder 3# sample, micro-or nano size cylinder 4# sample, micro-or nano size cylinder 5# sample is prepared successively through above-mentioned same method, and use nano-hardness tester to carry out the compression test of 11% deformation successively, the load-deformation curve obtained is as shown in Figure 11 to 14, from load-deformation curve, micro-or nano size cylinder 2# sample, micro-or nano size cylinder 3# sample, micro-or nano size cylinder 4# sample, micro-or nano size cylinder 5# sample reinforcement-
Basal body interface all ruptures；The sudden change stress value of above-mentioned each sample of nano-hardness tester record sees table 1, and the shear strength thus obtaining aluminum-base silicon carbide particulate reinforced composite is 133 ± 26Mpa.
The sudden change stress value of each sample of table 1
| Number | #1 | #2 | #3 | #4 | #5 | Average |
| ShearStress | 113Mpa | 108Mpa | 125Mpa | 153Mpa | 167Mpa | 133±26Mpa |
Test metal-base composites reinforcement and the method for matrix interface shear strength of the present invention, utilizes micro-nano mechanics method can directly record interface shear strength, overcomes the difficult problem that traditional method cannot directly record；Micro-or nano size cylinder design become the tilted interface the most at 45 ° with reinforcement-basal body interface shearing behavior can be made to be more prone to occur.
The Research Thinking that the present invention proposes is not limited to specific material system, can be extended in other materials more conveniently.Same Research Thinking can apply to actual macroscopic view bulk metal-base composites (i.e.: directly to carry out FIB etching on reinforcement granule and is through to body portion, obtain the composite minute yardstick cylinder sample containing reinforcement-basal body interface, and then it is compressed test), the design of intending in fact, model and optimize for actual macroscopic view block metal matrix composite provides strong experimental basis and theories integration.
Claims (7)
1. the method for testing of a metal-base composites shear strength, it is characterized in that, including: utilize focused-ion-beam lithography to go out the micro-or nano size cylinder (1) containing reinforcement-basal body interface, and the reinforcement-basal body interface (2) of this micro-or nano size cylinder (1) and this cylinder axially between there is certain angle, then nano-hardness tester is used axially to apply pressure along it at the end face of micro-or nano size cylinder (1), so that there is compressive deformation in micro-or nano size cylinder (1), reinforcement-basal body interface (2) will bear shearing force in the process, until shearing behavior will occur at reinforcement-basal body interface, the shear strength of reinforcement-basal body interface is calculated by the load-deformation curve of the micro-or nano size cylinder of nano-hardness tester record.
Method of testing the most according to claim 1, it is characterised in that described reinforcement-basal body interface (2) and this cylinder axially between angle be 45 °.
Method of testing the most according to claim 1, it is characterized in that, in test process, take to be gradually increased the method for pressure, and use under the conditions of scanning electron microscope, transmission electron microscope observing difference compression stress before and after compression experiment reinforcement-basal body interface and the Characteristics of Microstructure of microcell thereof in micro-or nano size cylinder sample, thus judge whether reinforcement-basal body interface lost efficacy.
4. a method of testing as claimed in claim 1, it is characterised in that comprise the steps:
A, select the metal-base composites of suitable dimension so that the size of the two phase material that reinforcement-basal body interface of being studied is corresponding can be used to prepare micro-or nano size cylinder, described reinforcement and matrix size and is in micron dimension；
B, use FIB etch there is independent reinforcement-basal body interface, this interface and cylinder axially have the micro-or nano size cylinder of certain angle；
The compression parameters that C, basis are preset, the tack pressure head of nano-hardness tester is used axially to apply certain pressure along it at the end face of micro-or nano size cylinder, carry out stress-strain test, use the reinforcement-basal body interface after tem observation deformation, it is judged that whether reinforcement-basal body interface lost efficacy；
D, it is stepped up compression parameters, by the experimental result comparison under the conditions of different compression parameters, the shear strength between reinforcement and basal body interface can be recorded more accurately, draw the shear strength of reinforcement and basal body interface according to the significantly stress-strain sudden change occurred on load-deformation curve.
Method of testing the most according to claim 4, it is characterized in that, in step B, described reinforcement-basal body interface (2) and this cylinder axially between angle be 45 °, the shear strength of described reinforcement-basal body interface is equal to a half value of the stress occurring catastrophe point on a large scale on load-deformation curve.
Method of testing the most according to claim 4, it is characterised in that in step B, described micro-or nano size column diameter be 200nm to 10 μm, draw ratio be 2:1～6:1, the tapering of micro-or nano size cylinder end face is not more than 3 °.
7. a micro-or nano size cylinder manufacture method as claimed in claim 2, it is characterised in that described metal-base composites is aluminum-base silicon carbide, uses wire cutting machine that 4H-SiC single-chip is cut into square pieces；According to ethanol, acetone, the sequencing of isopropanol, SiC single crystal small pieces are carried out ultrasonic cleaning, remove wafer surface impurity；SiC single crystal small pieces are immersed in melted Al liquid, propose after hand operated mixing, repeat above action until the thickness of Al layer is more than 1mm, prepare Al-SiC-Al sandwich structure composite；The one side selecting Al-SiC-Al sandwich structure composite sample is polished so that this face is smooth and Al aspect is parallel to SiC wafer；Composite sample after polishing is fixed on the wedge shape platform at 45 ° of inclination angles, and the one side of polishing is close to wedge shape microscope carrier；Sample parallel one side bottom wedge shape microscope carrier is polished, it is thus achieved that a plane being parallel to bottom.
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